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S'^is. "I 






IC 8885 



Bureau of Mines Information Circular/1982 




Characterization of U.S. Cement Kiln Dust 

By Benjamin W. Haynes and Gary W. Kramer 




UNITED STATES DEPARTMENT OF THE INTERIOR 



Information Circular 8885 



Characterization of U.S. Cement Kiln Dust 



By Benjamin W. Haynes and Gary W. Kramer 




UNITED STATES DEPARTMENT OF THE INTERIOR 
James G. Watt, Secretary 



BUREAU OF MINES 
Robert C. Horton, Director 



This publication has been cataloged as follows: 






Hayncs, Benjamin W 

Characterization of U.S. cement kiln dust. 

(Bureau of Mines information circular) 

Bibliography: p. 19. 

Supt. of Docs. No.: I 28.27:8885. 

1. Cement— Analysis. I. Kramer, Gary W. IF. Title. IH. Series: 
Information circular (United States. Bureau of Mines) ; 8885. 



-TP882TS7ftSa _ 666'. 94 82-600149 AACR2 



Bureau of Mines 
Information Circular 8885 






CHARACTERIZATION OF U.S. CEMENT KILN DUST 
By Benjamin W. Haynes and Gary W. Kramer 



ERRATA 
Page 2, first 3 lines of right-hand column should read as follows: 

EPA study of the cement industry concluded that: 
Page 6, .^ine 5 of right-hand column: 

3.8 should be 7.7 
Page 8, line 6 of right-hand coluraH: 

0.60 should be 0.68 

Page 17, table 10: 

Under Pb, delete -.44 
Under Sr, delete -0.77 

Page 18, line 4 of right-hand column: 

Expression in parentheses should be (r = 0.77). 






CONTENTS 

Page 

Abst ract 1 

Introduction 2 

Samples 2 

Mineralogy 3 

Chemical analyses 6 

Chemically bound water, carbon dioxide, and noncarbonate carbon. 6 

Anions 8 

Maj or , minor , and trace element s 8 

Interelement correlations 17 

EPA hazardous waste test 18 

Summary and conclusions 18 

References 19 

TABLES 

1 . Cement kiln dust samples received , by State 3 

2. Mineraloglcal composition of U.S. cement kiln 

dust samples 4 

3. Chemically bound water, CO2 , and noncarbonate 

carbon in U.S. cement kiln dust 7 

4. Anions in U.S. cement kiln dust 9 

5. Comparison of NBS SRM-637 certificate values with Bureau of 

Mines analytical method values 10 

6. Major and minor elements in U.S. cement kiln dust 11 

7. Trace elements in U.S. cement kiln dust 13 

8. Elemental and anion variation in U.S. cement kiln 

dust 16 

9. Mercury in selected U.S. cement kiln dust samples 17 

10. Interelement correlation coefficients for U. S. cement 

kiln dust 17 

11. Maximum concentration of contaminants allowed for 

EP toxicity test 18 



^ 



CHARACTERIZATION OF U.S. CEMENT KILN DUST 



By Benjamin W. Haynes^ and Gary W. Kramer'^ 



ABSTRACT 

Cement kiln dust (CKD) produced in the contiguous United States and 
Hawaii was characterized as part of the Bureau of Mines' program in 
minerals environmental technology. The mineralogical and chemical compo- 
sition was determined for 113 CKD samples from 102 plants that normally 
send CKD waste to landfill. Characterization included the determination 
of 28 elements, 7 anion species, carbon dioxide, noncarbonate carbon, and 
chemically bound water. Mercury was determined in 16 samples. Interele- 
ment correlation coefficients were determined for 23 elements, 5 anions, 
CO2, noncarbonate carbon, and chemically bound water. 

To assess the hazardous waste potential of CKD, the U.S. Environ- 
mental Protection Agency Extraction Procedure (EP) toxicity test was 
performed on all 113 CKD samples. All but one sample were in compliance 
with the test; the noncomplying sample slightly exceeded the EP toxicity 
test criterion for lead. 



^Supervisory research chemist, Avondale Research Center, Bureau of 

Mines, Avondale, Md. 
^Research chemist, Avondale Research Center, Bureau of Mines, Avondale, 
Md. 



INTRODUCTION 



Cement kiln dust (CKD) is a waste 
product that accumulates at the rate of 
4 to 12 million tons per year in the 
United States (2^, h)^ . This dust has 
considerable resource potential: It is 
already being used as a neutralizer for 
coal mine waste effluents, and the agri- 
cultural and construction industries are 
beginning to use it more extensively as 
a substitute for lime. In the proposed 
hazardous waste guidelines of 1978 iU) 
promulgated under the Resource Conserva- 
tion and Recovery Act (RCRA) of 1976 
(11), the Environmental Protection 
Agency (EPA) placed CKD in a "Special 
Wastes" category pending more informa- 
tion on the composition, characterist- 
ics, and degree of hazard posed by this 
waste. In 1980 the "Special Wastes" 
category was removed (5), but a 3-year 
EPA study of the hazard potential of 
CKD was approved by Congress (10 ) . Part 
of the concern over the environmental 
effects of waste CKD resulted from a 
single study of the heavy metals content 
of a CKD sample from Blaubeuren, West 
Germany, showing lead and zinc contents 
of 5,620 and 16,200 yg/g, respec- 
tively (3). The only other analysis of 
CKD for heavy metals used in the EPA 
study was sample from Polk County, Ga. , 
showing 124 Pg/g for lead and 145 
pg/g for zinc (12) . A contracted 



EPA study of the received in 1-gallon 
cans and prepared cement industry con- 
cluded that: 

Waste kiln dust is probably the most 
serious pollution control problem 
facing the cement industry at this 
time. Relatively little is known 
about the dust, so environmentally 
adequate management techniques are 
difficult to specify (2). 

An exploratory evaluation of the 
environmental effects and of the re- 
source recovery potential of the ele- 
ments present in CKD was initiated at 
the Bureau of Mines Avondale (Md.) Re- 
search Center shortly after publication 
of the 1978 EPA guidelines. Results of 
the first phase of this research (8), 
discussed major, minor, and trace ele- 
ment concentrations, mineralogy, anion 
composition, chemically bound water, 
CO2 , and EP toxicity leach test re- 
sults. The present report gives char- 
acterization data for the U.S. cement 
industry nationwide. Information on 
noncarbonate carbon has been added for 
all samples, as have mercury determina- 
tions on selected samples, and signifi- 
cant intereleraent correlation coeffici- 
ents for the major, minor, and trace 
elements. 



SAMPLES 



Samples of CKD were requested from 
operating plants located in the contigu- 
ous United States and Hawaii; 113 
samples from 102 plants, representing 
about 70 percent of the total U.S. 
cement industry, were received and ana- 
lyzed. The remaining plants either did 
not respond to the inquiry or had no 
disposal problems because all their 
waste dust was recycled. Table 1 lists 
the States and the number of samples 
received from each State. Samples were 
received in 1-gallon cans and prepared 



for analysis by the following proce- 
dure: 

1 . The sample as received was 
blended in a twin-shell blender for 30 
minutes, then riffle-split into two 
portions. 

2. One half of the sample was 
labeled and stored, and the other half 
was passed through a 100-mesh sieve. 
Any portion of the sample coarser than 
minus 100 mesh was ground in a Wiley 
mill^ to pass 100 mesh. 



3 Underlined numbers in parentheses refer 
to items in the list of references at 
the end of this report. 



"^Reference to specific brand names is 
made for identification only and does not 
imply endorsement by the Bureau of Mines. 



TABLE 1 . - Cement kiln dust samples received, by State^ 



State 


Number of 
samples 


State 


Number of 
samples 




State 


Number of 
samples 


Alabama 


4 
3 
2 
11 
4 
2 
1 
1 
1 
2 
2 
4 
5 


Kentucky 

Louisiana 

Maine 


1 
1 

3 
3 
1 
6 
1 
3 

1 
2 
1 




Ohio 


5 


Arizona 

Arkansas 


Oklahoma 

Oregon. 

Pennsylvania. . . 
South Carolina. 
South Dakota. . . 

Tennessee 

Texas 


3 

1 


California. . . 

Colorado 

Florida 

Georgia 

Hawaii 


Maryland 

Michigan 

Mississippi. . . . 

Missouri 

Montana 

Nebraska 

Nevada 

New Mexico 

New York 

North Carolina. 


9 

1 

3 

5 

14 


Idaho 

Illinois 

Indiana 

Iowa 

Kansas 


Utah 

Virginia 

Washington 

Wisconsin 

Wyoming 


1 
1 
4 

1 



•'^Only those States are listed that have cement plants in operation. 



3. The minus lOQ-mesh material 
(~ 1/2 gallon) was reblended for 
30 minutes. 

4. The sample was then riffle- 
split again into two fractions for char- 
acterization. 

All mineralogical and chemical ana- 
lysis data were obtained using the minus 



100-mesh material. The extraction pro- 
cedure (EP) toxicity leach test was 
performed on the blended as-received 
material. Samples were coded based on 
receipt date, and the tables of data 
have no correlation with the State 
listings in table 1. 



MINERALOGY 



Standard X-ray diffraction proce- 
dures using CuKa radiation were 
performed on the minus 100-mesh material 
to determine the minerals present. 
The results are given in table 2. All 
but seven samples contained calcite 
(CaCOg) as a major constituent, 
and those seven samples had calcite as a 
minor constituent. All but two samples 
contained quartz (Si02). Lime 

(CaO) and anhydrite (CaSO^) were 



present in most samples; amounts ranged 
from <5 to >30 wt-pct. Other minerals 
identified in the samples included aph- 
thitalite [(K,Na)2S0^, nine samples], 
arcanite (K2S0i^, nine samples), sylvite 
(KCl, nine samples), slaked lime 
[Ca(0H)2, six samples], halite (NaCl, 
one sample), and gypsum (CaSO^*2H20, one 
sample). Two samples contained low levels 
of chlorite [Mgg (Sii^OiQ )(0H)2'Mg3 (0H)g ] . 



TABLE 2. - Mineralogical composition of U.S. cement kiln dust samples^ 



Sample 


Calcite 


Lime 


Anhydrite 


Quartz 


Dolomite 


Mica 


Feldspar 


1 


Major 


Minor 


Minor 


Minor 


Minor 




Minor 


2 


Major 


Minor 


Very low 


Minor 








3 


Major 


Minor 


Low 


Low 


Minor 




Low 


4 


Major 


Minor 


Minor 


Low 


Low 


Very low 




5 


Major 


Minor 


Minor 


Low 


Very low 


Very low 




6 


Major 


Major 


Major 


Very low 








7 


Major 


Major 


Minor 


Low 






Low 


8 


Major 


Minor 


Low 


Low 


Low 




Minor 


9 


Major 




Low 


Low 


Low 


Very low 


Minor 


10 


Major 


Minor 


Minor 


Very low 


Low 


Very low 




11 


Major 


Minor 


Low 


Minor 








12 


Major 




Low 


Low 


Minor 


Very low 


Minor 


13 


Major 




Very low 


Low 


Minor 


Low 


Minor 


14 


Major 




Minor 


Low 


Minor 






15 


Major 


Minor 


Minor 


Minor 


Minor 






16 


Major 


Minor 


Low 


Low 


Low 






17 


Major 




Low 


Minor 


Low 




Low 


18 


Major 


Minor 


Minor 


Minor 








19 


Major 


Minor 


Minor 


Minor 


Minor 




Very low 


20 


Major 


Minor 


Low 


Very low 








21 


Major 


Minor 


Minor 


Low 


Minor 






22 


Major 


Low 


Minor 


Low 








23 


Major 




Low 


Very low 


Low 






24 


Major 


Low 


Low 


Low 


Low 






25 


Minor 


Major 




Low 








26 


Major 


Minor 


Minor 


Very low 








27 


Major 


Minor 


Low 


Low 








28 


Major 


Low 




Low 








29 


Major 


Minor 




Low 








30 


Major 


Minor 


Minor 


Low 


Low 






31 


Major 




Very low 


Low 








32 


Major 


Minor 


Low 


Low 








33 


Major 


Low 


Low 


Very low 








34 


Major 


Minor 


Low 


Low 








35 


Major 


Minor 


Minor 


Low 








36 


Major 


Minor 


Minor 


Very low 








37 


Major 


Low 


Minor 


Very low 


Low 






38 


Major 


Very low 




Low 


Low 






39 


Major 


Minor 


Low 


Low 


Low 






40 


Major 


Minor 




Very low 


Low 






41 


Major 


Minor 


Low 


Very low 








42 


Major 


Major 


Minor 


Very low 








43 


Major 


Minor 


Minor 


Very low 








44 


Major 


Very low 


Minor 


Very low 


Very low 






45 


Major 


Very low 


Very low 


Very low 








46 


Minor 






Very low 




Very low 




47 


Major 


Low 


Low 


Very low 


Low 






48 


Major 






Very low 




Very low 





^See footnotes at end of table, 



TABLE 2. - Mineralogical composition of U.S. cement kiln dust samples 
— Continued 



Sample 


Calcite 


Lime 


A.nhydrite 


Quartz 


Dolomite 


Mica 


Feldspar 


49 


Major 




Low 


Very low 


Low 






50 


Major 






Very low 








51 


Major 


Very low 


Low 


Very low 


Very low 






52 


Major 


Minor 


Low 


Very low 








53 


Major 


Low 


Low 


Low 




Very low 




54 


Major 


Minor 




Very low 


Low 


Very low 




55 


Major 


Major 


Very low 


Very low 


Very low 






56 


Major 


Minor 


Very low 


Low 


Low 




Low 


57 


Major 






Very low 




Very low 




58 


Major 






Very low 


Low 






59 


Major 


Low 


Low 


Very low 








60 


Major 


Low 


Low 


Very low 


Low 






61 


Major 


Low 


Low 


Very low 








62 


Major 


Minor 


Low 


Very low 


Low 






63 


Major 






Very low 


Low 






64 


Major 


Major 




Very low 


Very low 






65 


Major 




Low 


Very low 


Minor 






66 


Major 


Low 


Low 


Very low 


Low 






67 


Major 






Very low 


Low 






68 


Major 






Very low 








69 


Major 


Low 




Very low 


Low 






70 


Major 


Low 




Very low 








71 


Major 


Minor 


Very low 


Very low 








72 


Major 


Minor 




Low 








73 


Major 


Low 


Very low 


Very low 








74 


Major 


Low 


Low 




Low 






75 


Major 


Minor 


Low 


Very low 








76 


Major 






Low 


Low 






77 


Major 


Minor 


Low 


Low 








78 


Major 


Low 


Very low 


Low 




Very low 




79 


Major 


Very low 


Low 


Low 


Very low 






80 


Major 


Minor 




Low 




Very low 




81 


Major 


Very low 




Very low 








82 


Major 


Minor 




Very low 






Low 


83 


Major 


Minor 


Low 


Very low 








84 


Major 


Minor 


Very low 


Very low 








85 


Major 


Very low 




Very low 






Very low 


86 


Major 


Minor 


Low 


Very low 








87 


Major 


Low 


Low 


Very low 


Very low 






88 


Major 


Low 




Very low 








89 


Major 


Low 




Low 








90 


Minor 


Major 


Minor 


Very low 








91 


Minor 


Major 


Low 


Very low 








92 


Major 


Minor 


Very low 


Very low 






Minor 


93 


Major 


Low 


Low 


Very low 








94 


Major 


Low 




Very low 









See footnotes at end of table. 



TABLE 2. - Mineralogical composition of U.S. cement kiln dust samples-*- 





— Continued 








Sample 


Calcite 


Lime 


Anhydrite 


Quart z 


Dolomite 


Mica 


Feldspar 


95 


Major 


Minor 


Minor 










96 


Major 


Low 


Low 


Low 




Very low 




97 


Major 


Low 


Low 


Very low 








98 


Major 




Very low 


Low 




Very low 




99 


Major 


Low 


Low 


Very low 








100 


Major 


Very low 




Very low 








101 


Major 


Minor 


Very low 


Very low 




Very low 




102 


Minor 


Major 


Low 


Very low 








103 


Major 


Low 


Low 


Low 








104 


Major 


Minor 




Low 








105 


Major 


Low 




Very low 








106 


Major 


Minor 


Very low 


Very low 








107 


Major 




Very low 


Very low 








108 


Low 


Major 


Very low 


Very low 








109 


Major 




Minor 


Very low 








110 


Major 


Low 


Low 


Very low 








111 


Major 


Low 


Low 


Low 


Low 






112 


Major 


Minor 




Low 








113 


Very low 


Major 




Very low 









Major 
Minor 
Low 



>30 wt-pct. 
10-30 wt-pct. 
5-10 wt-pct. 



Very low 
Blank 



<5 wt-pct. 
Not detected. 



'^Analysis by C. W. Huggins, research chemist, Avondale Research Center, Bureau 
of Mines, Avondale, Md. 

CHEMICAL ANALYSES 



The chemical analyses of the CKD 
samples are discussed in three sections 
as follows: (1) Chemically bound water, 
carbon dioxide and noncarbonate carbon 
concentrations; (2) anion concentra- 
tions; and (3) major, minor, and trace 
element concentrations. The samples 
used for the analyses were the blended 
minus 100-mesh materials. 

Chemically Bound Water, Carbon 
Dioxide, and Noncarbonate Carbon 

The amount of chemically bound 
water and carbon dioxide (CO2) present 
in CKD was determined using thermogravi- 
metrtc analysis (TGA). Chemically bound 
water and CO2 are defined as the water 
and CO2 requiring temperatures greater 



than 110° C to expel them from the 
material being analyzed. The results of 
the TGA analyses are shown in table 3. 
Chemically bound water was low in all 
samples, ranging from 0.4 to 3.8 
wt-pct. The CO2 content ranged from 
4.4 to 34.4 wt-pct. No data are report- 
ed for chemically bound water and CO2 
for samples 17, 46, 57-59, 72, 82, and 
84 because under the high-temperature, 
low-vacuum conditions of the analysis, 
vapors from the samples repeatedly 
corroded the 20-mil platinum- rhodium 
hangdown wire to the breaking point 
before the determination could be made. 
These samples contained high levels of 
sylvite (KCl), which attacks platinum- 
rhodium alloys. 



TABLE 3 . - Chemically bound water, CO^ , and noncarbonate carbon in U.S. cement 
kiln dust, wt-pct 





Chemically 




Noncar- 




Chemically 




Noncar- 


Sample 


bound 


C02^ 


bonate 


Sample 


bound 


C02^ 


bonate 




water ^ 




carbon 




water ^ 




carbon 


1 


0.7 


22.3 


0.41 


46 


ND 


ND 


1.83 


2 


.4 


23.8 


.51 


47 


1.2 


22.9 


.19 


3 


.8 


19.4 


1.01 


48 


1.0 


22.9 


.44 


4 


1.9 


26.5 


.62 


49 


.8 


30.2 


.21 


5 


1.3 


24.2 


.78 


50 


1.1 


34.4 


.32 


6 


.4 


8.0 


.50 


51 


2.9 


16.5 


.82 


7 


.4 


8.8 


.56 


52 


1.0 


20.5 


.10 


8 


.4 


17.5 


.50 


53 


1.0 


21.0 


.26 


9 


.8 


21.9 


.58 


54 


1.3 


27.3 


.61 


10 


1.3 


22.6 


1.00 


55 


1.5 


19.2 


.20 


11 


.9 


19.1 


.42 


56 


1.4 


26.0 


.48 


12 


1.1 


19.6 


.41 


57 


ND 


ND 


.54 


13 


1.3 


23.7 


.18 


58 


ND 


ND 


.53 


14 


1.1 


21.7 


.65 


59 


ND 


ND 


<.01 


15 


.8 


12.4 


.85 


60 


2.1 


18.1 


.78 


16 


1,0 


23.9 


.05 


61 


.9 


22.0 


.23 


17 


ND 


ND 


.75 


62 


1.5 


26.4 


1.40 


18 


1.3 


19.6 


.74 


63 


.8 


34.2 


1.22 


19 


.7 


29.4 


1.23 


64 


1.0 


13.5 


.56 


20 


1.2 


26.2 


.68 


65 


1.1 


22.2 


.41 


21 


.9 


27.1 


.70 


66 


2.0 


19.0 


1.00 


22 


2.0 


20.6 


.32 


67 


2.0 


25.1 


.41 


23 


.7 


10.4 


.54 


68 


3.8 


23.0 


.72 


24 


1.8 


23.5 


.23 


69 


1.4 


22.2 


1.02 


25 


1.4 


14.3 


.49 


70 


.6 


25.1 


1.63 


26 


1.8 


16.8 


.38 


71 


1.5 


20.8 


.54 


27 


.8 


15.2 


.77 


72 


ND 


ND 


.44 


28 


1.1 


27.7 


<.01 


73 


1.0 


30.9 


.51 


29 


.9 


23.8 


.44 


74 


1.1 


25.9 


1.10 


30 


1.0 


31.3 


.61 


75 


1.1 


20.7 


.42 


31 


2.9 


24.3 


.23 


76 


1.0 


33.2 


<.01 


32 


1.4 


24.3 


.52 


77 


1.3 


13.0 


.40 


33 


1.3 


19.8 


.46 


78 


1.2 


30.1 


.29 


34 


1.1 


23.8 


.66 


79 


2.5 


21.8 


.12 


35 


3.0 


17.1 


.39 


80 


1.5 


23.3 


.55 


36 


2.0 


20.7 


.30 


81 


1.5 


12.6 


.07 


37 


1.1 


24.0 


.49 


82 


ND 


ND 


<.01 


38 


1.1 


32.6 


.71 


83 


.7 


26.0 


.88 


39 


1.0 


26.5 


.77 


84 


ND 


ND 


.45 


40 


1.1 


22.1 


.78 


85 


1.6 


28.3 


.24 


41 


.9 


25.9 


1.60 


86 


1.0 


17.9 


.62 


42 


1.0 


19.2 


.97 


87 


1.6 


22.4 


.19 


43 


1.1 


20.4 


.98 


88 


.7 


18.3 


.03 


44 


1.2 


25.2 


.84 


89 


1.0 


24.0 


.14 


45 


2.1 


20.0 


.99 


90 


1.0 


15.3 


.20 



•See footnotes at end of table, 



TABLE 3. - Chemically bound water, C02» and noncarbonate carbon In U.S« cement kiln 
dust, wt-pct — Continued 





Chemically 




Noncar- 




Chemically 




Noncar- 


Sample 


bound 


CO2 


bonate 


Sample 


bound 


CO2 


bonate 




water 




carbon 




water 




carbon 


91 


1.8 


12.0 


0.15 


103 


2.8 


22.4 


0.18 


92 


1.2 


27.0 


.17 


104 


1.3 


25.1 


.86 


93 


1.8 


19.1 


.25 


105 


1.2 


26.6 


.23 


94 


.9 


15.4 


.15 


106 


1.4 


23.0 


.21 


95 


1.3 


20.6 


.06 


107 


1.0 


31.7 


.56 


96 


1.3 


24.0 


.23 


108 


2.4 


4.4 


.34 


97 


1.7 


23.8 


.11 


109 


3.0 


21.9 


.70 


98 


1.9 


23.8 


.13 


110 


1.4 


20.5 


1.23 


99 


1.1 


33.3 


.44 


HI 


.5 


31.5 


.44 


100 


1.3 


23.3 


.11 


112 


.9 


23.7 


.33 


101 


1.0 


21.8 


.24 


113 


.8 


8.2 


.45 


102 


7.7 


8.7 


.64 











ND Not determined. 

^Analysis by J. V. Scalera, chemist, Avondale Research Center, Bureau of Mines, 
Avondale, Md. 



Noncarbonate carbon was determined 
by treating a weighed sample with dilute 
HCl and heating to dissolve the carbon- 
ate minerals present (calcite, dolo- 
mite.) After evolution of CO2 ceased, 
the samples were rinsed to remove excess 
acid and analyzed by a LECO carbon ana- 
lyzer. Noncarbonate carbon is generally 
unburned coal or fuel oil in the CKD 
samples. The concentrations as shown in 
table 3 ranged from <0.01 to 1.83 
wt-pct . 

Anions 

The anion species present in the CKD 
samples were determined using a Dionex 
10 ion chromatograph. The CKD samples 
were weighed and then fused with 
Na2C03. After fusion, the samples 

were leached with high purity deionized 
distilled water and diluted to a stand- 
ard concentration; and aliquots of a 
1-to-lO dilution were injected into Che 
ion chromatograph. 

Details of this procedure are given 
elsewhere (7^). Determinations of chlo- 
ride (Cl~), fluoride (F~) , nitrate 
(N03~), phosphate (PO43-) , and 



sulfate (S04^~) were obtained from 
a single sample injection. The results 
of these determinations on the U. S. CKD 
samples are presented in table 4. Chlo- 
ride ranged from <0.01 to 12.3 wt-pct, 
fluoride from 0.01 to 0.60 wt-pct, 
nitrate from <0.02 to 1.67 wt-pct, phos- 
phate from <0.02 to 0.16 wt-pct, and 
sulfate from 0.41 to 31.6 wt-pct. Bro- 
mide (Br~) and nitrite (N02~) can 
also be determined by this method from 
the same injection of solution, but no 
samples were found to contain either 
Br~ or N02~ at levels greater than 
the detection limit (<0.02 wt-pct) for 
these anions. 

Major, Minor, and Trace Elements 

The elements Al, Si, K, Ca, Ti, and 
Fe were determined for the majority of 
samples by a f used-disk. fluorescent 
X-ray spectrography procedure. Fifteen 
CKD samples were analyzed for the above 
elements by wet chemical techniques, and 
these samples were used as secondary 
standards for the X-ray method. Other 
major, minor, and trace elements were 
determined by flame atomic absorption 
spectroscopy (AAS). Samples were 



TABLE 4. - Anions In U.S. cement kiln dust, wt-pct 











3- 


2- 






' 




3- 


2- 


Sample 


CI 


F 


NO 


f°4 


SO, 


Sample 


CI 


F 


NO3- 


P°4 


so/ 


1 


0.01 


0.13 


0.76 


<0.02 


9.77 


58 


1.03 


0.06 


<0.02 


<0.02 


2.02 


2 


.04 


.08 


.05 


.05 


2.63 


59 


1.09 


.09 


<.02 


<.02 


10.8 


3 


.90 


.09 


.32 


<.02 


9.06 


60 


.35 


.16 


<.02 


<.02 


10.6 


4 


.18 


.13 


.11 


.05 


7.43 


61 


.89 


.12 


<.02 


.02 


8.21 


5 


.10 


.14 


.23 


.05 


7.93 


62 


.19 


.04 


.12 


<.02 


6.63 


6 


.04 


.36 


.32 


.08 


12.2 


63 


.16 


.06 


<.02 


<.02 


1.15 


7 


.66 


.31 


.23 


.02 


12.4 


64 


.24 


.26 


.07 


<.02 


2.64 


8 


1.93 


.10 


.09 


<.02 


19.2 


65 


.29 


.08 


<.02 


<.02 


19.8 


9 


5.18 


.07 


1.00 


<.02 


12.0 


66 


.40 


.12 


<.02 


<.02 


10.8 


10 


.42 


.26 


.37 


.05 


7.95 


67 


.13 


.14 


<.02 


.02 


3.56 


U 


<.01 


.05 


<.02 


<.02 


4.15 


68 


.26 


.20 


<.02 


<.02 


5.38 


12 


.17 


.22 


.21 


<.02 


10.7 


69 


.06 


.04 


<.02 


<.02 


4.26 


13 


.52 


.04 


.23 


.10 


14.7 


70 


.13 


.68 


<.02 


.02 


6.29 


14 


.18 


.10 


.05 


<.02 


18.6 


71 


.52 


.05 


.07 


<.02 


2.60 


15 


<.01 


.23 


<.02 


<.02 


14.2 


72 


3.32 


.15 


<.02 


<.02 


3.73 


16 


.21 


.12 


.56 


.10 


4.96 


73 


.58 


.08 


<.02 


<.02 


2.22 


17 


.89 


.09 


.09 


<.02 


6.05 


74 


.59 


.05 


<.02 


.02 


6.59 


la 


1.17 


.20 


.23 


.16 


4.91 


75 


.63 


.11 


<.02 


<.02 


7.42 


19 


.57 


.03 


.19 


<.02 


12.4 


76 


.48 


.10 


<.02 


.03 


6.02 


20 


.19 


.08 


1.67 


.03 


10.4 


77 


.49 


.25 


<.02 


<.02 


10.7 


21 


.56 


.11 


.10 


<.02 


7.27 


78 


.38 


.05 


<.02 


<.02 


.82 


22 


.38 


.12 


.12 


<.02 


10.5 


79 


.62 


.07 


<.02 


<.02 


7.52 


23 


.40 


.35 


<.02 


<.02 


31.6 


80 


.35 


.07 


<.02 


.03 


2.29 


24 


.12 


.16 


<.02 


<.02 


3.77 


81 


1.20 


.20 


.11 


.02 


21.5 


25 


.04 


.13 


<.02 


<.02 


1.66 


82 


.70 


.19 


<.02 


<.02 


12.5 


26 


.15 


.09 


<.02 


<.02 


10.9 


83 


.51 


.10 


<.02 


<.02 


7.59 


27 


1.01 


.05 


<.02 


<.02 


6.63 


84 


1.36 


.19 


<.02 


<.02 


3.48 


28 


.28 


.11 


<.02 


<.02 


9.52 


85 


.49 


.15 


<.02 


<.02 


.41 


29 


.35 


.11 


.74 


<.02 


6.16 


86 


.55 


.16 


<.02 


<.02 


11.6 


30 


.15 


.15 


<.02 


<.02 


6.27 


87 


.51 


.14 


<.02 


<.02 


5.12 


31 


1.13 


.14 


<.02 


<.02 


5.85 


88 


.52 


.22 


.09 


.02 


6.51 


32 


.45 


.04 


<.02 


<.02 


.86 


89 


.38 


.12 


<.02 


<.02 


3.83 


33 


1.97 


.01 


<.02 


<.02 


1.83 


90 


.57 


.16 


<.02 


<.02 


12.3 


34 


.47 


.10 


.15 


<.02 


5.31 


91 


.86 


.20 


<.02 


<.02 


6.61 


35 


.41 


.05 


.41 


<.02 


5.72 


92 


.38 


.04 


<.02 


<.02 


3.80 


36 


.49 


.10 


<.02 


<.02 


8.01 


93 


.42 


.16 


<.02 


.02 


7.68 


37 


.51 


.07 


.15 


<.02 


7.20 


94 


.39 


.19 


<.02 


<.02 


6.16 


38 


.82 


.09 


<.02 


<.02 


.61 


95 


.42 


.07 


<.02 


<.02 


10.2 


39 


.31 


.06 


.23 


<.02 


2.35 


96 


.49 


.10 


<.02 


<.02 


5.42 


40 


.78 


.18 


.18 


<.02 


5.46 


97 


.25 


.13 


<.02 


<.02 


6.12 


41 


.52 


.12 


<.02 


<.02 


4.85 


98 


.80 


.06 


<.02 


<.02 


7.15 


42 


.13 


.14 


<.02 


<.02 


8.37 


99 


.42 


.05 


<.02 


<.02 


3.70 


43 


.58 


.13 


<.02 


.02 


15.7 


100 


.46 


.29 


.07 


<.02 


9.16 


44 


.44 


.07 


<.02 


<.02 


10.8 


101 


.47 


.20 


<.02 


<.02 


3.38 


45 


.11 


.09 


<.02 


<.02 


5.68 


102 


.16 


.09 


<.02 


<.02 


5.31 


46 


12.3 


.05 


<.02 


<.02 


31.5 


103 


.87 


.09 


<.02 


<.02 


5.92 


47 


.84 


.12 


<.02 


<.02 


9.05 


104 


.43 


.11 


<.02 


<.02 


2.13 


48 


.82 


.04 


.07 


<.02 


1.01 


105 


1.00 


.09 


<.02 


<.02 


3.42 


49 


.73 


.05 


.07 


.02 


2.86 


106 


1.32 


.13 


<.02 


<.02 


4.84 


50 


.48 


.07 


<.02 


.04 


.49 


107 


.35 


.07 


<.02 


<.02 


2.21 


51 


.39 


.20 


<.02 


<.02 


15.3 


108 


1.84 


.16 


<.02 


<.02 


14.0 


52 


.52 


.05 


<.02 


<.02 


6.43 


109 


.71 


.05 


.16 


<.02 


13.9 


53 


.36 


.07 


<.02 


<.02 


7.15 


110 


.47 


.16 


<.02 


.02 


11.8 


54 


.31 


.09 


<.02 


<.02 


4.04 


111 


.21 


.14 


<.02 


<.02 


2.92 


55 


.34 


.12 


<.02 


<.02 


6.86 


112 


.22 


.31 


<.02 


<.02 


2.30 


56 


.39 


.10 


<.02 


<.02 


1.70 


113 


2.56 


.40 


<.02 


<.02 


5.22 


57 


.72 


.33 


<.02 


<.02 


22.0 















10 



prepared for AAS analysis by dissolving 
2 grams of CKD sample in a mixture of 10 
ml concentrated HNO3, 5 ml HF, and 40 
ml distilled H2O . The sample was evap- 
orated to dryness. The dried sample was 
redissolved in 5 vol-pct HNO3 to which 
5 ml of 30-pct H2O2 was added. The 
solution was gently heated and, after 
the H2O2 reaction had subsided, 5 to 
10 ml of concentrated HCl was added to 
dissolve the remaining solids. The 
samples were cooled and transferred to 
volumetric flasks for AAS analysis. 

Arsenic and antimony were determined 
by a reliable graphite furnace AAS 
method developed by the Bureau of Mines 
(6, 9). Mercury was determined using 
the method of Ageraian and Chau (1) as 
modified by Haynes (9) . 

Duplicate analyses were performed on 
all CKD samples. To verify the results 
obtained by chemical dissolutions, the 
flame AAS procedure, and other proce- 
dures used in this report, a National 
Bureau of Standards (NBS) Standard 
Reference Material (SRM) cement stand- 
ard, SRM-637, was analyzed, and these 
values were compared with certificate 
results. The results are listed in 
table 5 and show good agreement between 
certified values and values obtained by 
the methods used in this study. 

The results for the major and minor 
element concentration [arbitrarily 
chosen as greater than 0.05 wt-pct (500 
Ug/g)] are given in table 6. Table 7 
gives the trace element concentration 
[arbitrarily selected as less than 0.05 
wt-pct (500 ug/g)] . 

Also listed in table 7 are seven 
elements, and their detection limits, 
that were not detected by flame atomic 
absorption in any of the samples. Twen- 
ty-eight elements were examined in all 
of the samples. Thallium was detected 
in only one sample, at 185 Ug/g. 
The presence of thallium in sample 9, as 
determined by flame AAS, was verified by 
fluorescent X-ray spectrography and 
optical emission spectroscopic techni- 
ques. 



TABLE 5. - Comparison of NBS SRM-637 
certificate values with Bureau of 
Mines analytical method values, wt-pct 



Constituent 



CaO. . , 
Si02. , 
AI2O3, 
Fe203, 
SO3. . , 
MgO.., 
K2O. . . 
Ti02 . , 
Na20. , 
SrO. . , 

P2O5.. 
Mn203 , 

F 

ZnO . . , 
Cr203. 



Concentration 



65 


.8 


23 


.2 


3 


.15 


1 


.72 


2 


.28 




.62 




.22 




.21 




.13 




.08 




.22 




.06 




.04 




.01 




.01 



Certified 
value^ 



66.0(4) 

23.0(7) 

3.2(8) 

1.80 

2.3(8) 

.6(7) 

.25 

.21 

.15 

.09 

.24 

.06 

.04 

.01 

.01 



Iparentheses indicate estimated level 
by NBS of next digit. 



Table 8 lists the range, arithmetic 
mean, and median found for each element 
in the 113 CKD samples. Ranges over 
three orders of magnitude are seen for 
some elements. The median may indicate 
the most probable value for the CKD 
samples where an anomalously high or low 
value for an element was found in one of 
the samples. Except for Ca, Ni, and Si, 
the median is lower than the mean for 
each element, indicating that the high 
concentrations are less frequent than 
the lower concentrations. 

Because traces of mercury were 
leached from only a few samples by the 
EP toxicity test, these samples and a 
few additional samples were chosen to 
insure an adequate geographic 
representation of the plants in the 
United States. Table 9 gives the results 
of analysis of 16 samples chosen by the 
above procedure. Mercury was determined 
by standard cold vapor AAS procedures 
(1, 9). 



11 



TABLE 6 . - Major and minor elements in U.S. cement kiln dust, wt-pct 



Sample 


Al 


Ca 


Fe 


K 


Mg 


Na 


Si 


Sr 


Ti 


1 


1.74 


31.6 


1.41 


1.96 


1.76 


0.73 


6.68 


0.02 


0.12 


2 


2.05 


36.1 


1.58 


.68 


.87 


.50 


5.29 


.02 


.16 


3 


2.66 


31.8 


1.51 


5.04 


.37 


.47 


6.33 


.04 


.14 


4 


2.89 


29.4 


1.38 


2.50 


1.39 


.45 


6.63 


.08 


.13 


5 


2.71 


32.8 


1.17 


1.50 


1.16 


.42 


5.72 


.08 


.12 


6 


3.82 


32.0 


3.61 


3.73 


.96 


.45 


7.62 


.17 


.20 


7 


3.40 


27.3 


2.58 


3.65 


1.21 


.54 


7.16 


.18 


.16 


8 


1.69 


22.2 


1.10 


11.9 


.68 


.59 


4.14 


.02 


.09 


9 


2.37 


19.8 


1.03 


8.78 


1.01 


.96 


4.93 


.04 


.10 


10 


3.99 


24.0 


2.24 


4.16 


1.12 


.57 


6.24 


.08 


.20 


11 


2.61 


34.1 


2.53 


1.10 


.70 


.19 


8.64 


.04 


.13 


12 


2.58 


29.2 


1.48 


3.53 


1.91 


1.18 


6.93 


.08 


.12 


13 


2.44 


23.6 


1.39 


5.99 


1.59 


.91 


4.13 


.08 


.13 


14 


1.71 


23.9 


.89 


6.89 


1.26 


1.15 


4.35 


.17 


.09 


15 


2.53 


30.3 


1.81 


5.95 


1.10 


.58 


7.09 


.07 


.12 


16 


2.21 


33.7 


1.35 


2.43 


1.01 


.62 


6.93 


.04 


.14 


17 


2.50 


30.5 


1.31 


3.53 


.63 


.48 


5.90 


.03 


.11 


18 


5.02 


21.3 


2.39 


2.01 


.31 


1.44 


11.1 


.50 


.29 


19 


2.07 


31.5 


1.62 


2.68 


.35 


.98 


6.00 


.07 


.14 


20 


2.34 


33.5 


1.41 


2.21 


.48 


.50 


5.31 


.04 


.13 


21 


1.97 


30.5 


1.83 


1.66 


1.46 


.30 


7.79 


.05 


.11 


22 


2.50 


28.5 


1.50 


2.42 


.81 


.44 


8.16 


.03 


.13 


23 


1.44 


11.3 


2.29 


15.1 


.34 


2.36 


3.30 


.02 


.07 


24 


3.22 


26.7 


1.94 


2.79 


1.56 


.20 


8.94 


.04 


.16 


25 


2.10 


34.5 


1.64 


2.11 


1.10 


.25 


7.33 


.06 


.11 


26 


2.58 


31.6 


2.37 


1.43 


.66 


.21 


6.83 


.04 


.10 


27 


2.05 


31.6 


1.18 


2.43 


1.02 


.16 


7.65 


.01 


.10 


28 


1.92 


28.7 


1.11 


4.34 


.56 


.48 


4.90 


.02 


.09 


29 


1.80 


33.0 


1.35 


1.77 


.64 


.23 


7.40 


.02 


.08 


30 


1.86 


33.2 


1.03 


1.86 


1.35 


.09 


5.53 


.01 


.11 


31 


1.95 


30.7 


1.22 


2.19 


.34 


.89 


8.02 


.22 


.11 


32 


2.54 


33.2 


1.72 


.72 


.29 


.15 


8.71 


.01 


.13 


33 


2.99 


32.7 


1.50 


2.56 


.31 


.20 


5.63 


.12 


.16 


34 


2.62 


31.8 


1.81 


2.47 


.30 


.18 


7.56 


.05 


.10 


35 


2.45 


33.8 


1.77 


.61 


.35 


.18 


7.53 


.11 


.10 


36 


2.01 


32.0 


1.68 


2.35 


.46 


.30 


6.51 


.07 


.09 


37 


2.64 


28.4 


1.60 


3.05 


1.17 


.30 


8.20 


.04 


.13 


38 


1.84 


31.6 


.98 


1.84 


1.66 


.05 


6.55 


.03 


.08 


39 


2.04 


33.4 


.91 


1.69 


1.38 


.22 


6.72 


.02 


.10 


40 


2.63 


30.9 


1.43 


2.55 


.79 


.07 


7.13 


.05 


.13 


41 


2.11 


34.6 


1.42 


.86 


.69 


.32 


6.16 


.10 


.10 


42 


2.11 


34.6 


1.42 


.86 


1.48 


.18 


6.16 


.05 


.10 


43 


2.52 


27.3 


1.33 


5.51 


.31 


.48 


5.63 


.08 


.12 


44 


2.03 


28.3 


1.30 


3.72 


.84 


.38 


6.17 


.02 


.12 


45 


2.32 


27.2 


1.56 


5.04 


.64 


.77 


6.72 


.12 


.12 


46 


.99 


10.6 


.66 


23.2 


.24 


.71 


3.60 


.01 


.06 



12 



TABLE 6 . - Major and minor elements In U.S. cement kiln dust, wt-pct 
— Continued 



Sample 


Al 


Ca 


Fe 


K 


Mg 


Na 


Si 


Sr 


Ti 


47 


2.50 


28.4 


1.65 


3.53 


1.20 


0.40 


7.07 


0.02 


0.16 


48 


2.23 


33.2 


1.27 


1.02 


.66 


.14 


5.72 


.03 


.13 


49 


1.90 


33.1 


1.36 


1.11 


1.24 


.12 


6.51 


.02 


.16 


50 


2.26 


36.0 


1.00 


.67 


.34 


.10 


5.20 


.05 


.11 


51 


2.12 


27.3 


1.10 


5.16 


.30 


.43 


4.97 


.08 


.10 


52 


1.97 


31.7 


1.60 


3.05 


.41 


.25 


6.51 


.02 


.07 


53 


2.40 


30.3 


1.49 


2.82 


.82 


.33 


6.89 


.06 


.14 


54 


2.62 


31.2 


1.16 


3.58 


.76 


.22 


4.95 


.05 


.12 


55 


2.26 


34.4 


1.01 


3.36 


.77 


.15 


3.65 


.05 


.09 


56 


2.10 


30.5 


1.27 


1.12 


.98 


.30 


5.31 


.04 


.10 


57 


2.07 


13.3 


1.03 


19.8 


.57 


.51 


3.17 


.03 


.09 


58 


2.36 


28.4 


1.32 


3.42 


.78 


.20 


5.78 


.05 


.12 


59 


1.87 


27.8 


1.07 


3.69 


.70 


.34 


5.98 


.08 


.09 


60 


2.14 


26.4 


1.26 


5.22 


1.07 


.76 


6.19 


.04 


.12 


61 


2.16 


27.2 


2.03 


5.19 


.49 


.35 


6.20 


.02 


.11 


62 


2.14 


34.5 


1.16 


1.87 


.80 


.49 


5.08 


.01 


.11 


63 


2.35 


33.8 


1.01 


1.28 


.65 


.09 


5.66 


.02 


.12 


64 


2.72 


34.1 


1.41 


3.80 


.54 


.45 


5.83 


.07 


.12 


65 


1.72 


21.5 


.75 


11.0 


.65 


.76 


2.72 


.03 


.09 


66 


2.60 


28.7 


2.50 


3.98 


.53 


.42 


5.90 


.03 


.11 


67 


2.78 


28.0 


1.41 


3.77 


1.42 


.68 


7.28 


.04 


.14 


68 


1.92 


27.0 


.90 


6.47 


1.33 


.88 


5.69 


.04 


.11 


69 


1.98 


31.6 


1.52 


2.25 


1.06 


.58 


7.31 


.02 


.09 


70 


1.37 


25.7 


.79 


11.6 


.52 


2.32 


2.69 


.02 


.06 


71 


1.67 


35.8 


2.32 


.34 


.26 


.15 


7.00 


.03 


.07 


72 


2.30 


27.3 


1.93 


4.46 


.43 


2.77 


7.25 


.88 


.11 


73 


2.19 


33.4 


1.26 


1.64 


.91 


.27 


5.39 


.07 


.09 


74 


2.31 


31.4 


1.28 


1.80 


.52 


.30 


7.25 


.01 


.12 


75 


2.33 


25.8 


1.51 


2.58 


.81 


.20 


5.54 


.07 


.13 


76 


1.92 


33.0 


.98 


.97 


.80 


.22 


6.49 


.07 


.09 


77 


1.82 


29.1 


2.00 


3.09 


.84 


.47 


7.68 


.04 


.08 


78 


2.43 


33.4 


1.18 


.65 


.56 


.22 


7.09 


.02 


.12 


79 


2.72 


29.4 


1.77 


2.19 


.81 


.42 


7.43 


.22 


.14 


80 


1.72 


34.9 


1.59 


1.07 


.63 


.28 


7.12 


.01 


.10 


81 


2.63 


19.4 


1.59 


10.1 


.34 


1.11 


5.70 


.07 


.13 


82 


2.12 


27.1 


.10 


5.52 


.65 


1.09 


6.27 


.02 


.05 


83 


1.83 


31.5 


1.65 


2.53 


.60 


.37 


5.80 


.06 


.08 


84 


1.85 


33.1 


1.04 


2.16 


.49 


.38 


6.37 


.08 


.10 


85 


2.51 


29.2 


1.51 


5.29 


.20 


.58 


6.36 


.06 


.12 


86 


2.40 


29.2 


.94 


5.56 


.22 


.27 


6.97 


.03 


.11 


87 


2.46 


32.0 


1.52 


2.48 


.62 


.21 


6.88 


.02 


.12 


88 


2.28 


26.5 


1.16 


6.38 


1.05 


.99 


7.40 


.02 


.11 


89 


2.49 


31.5 


1.77 


2.17 


.59 


.20 


7.35 


.08 


.13 


90 


2.98 


28.7 


2.27 


3.92 


.67 


.29 


7.79 


.03 


.15 


91 


2.58 


31.8 


1.38 


3.27 


1.52 


.26 


6.26 


.02 


.12 


92 


1.93 


35.1 


1.26 


.96 


.27 


.36 


5.71 


.06 


.09 


93 


2.54 


30.5 


2.02 


2.65 


.43 


.23 


6.86 


.17 


.11 



13 



TABLE 6. - Major and minor elements in U.S. cement kiln dust, wt-pct 
— Continued 



Sample 


Al 


Ca 


Fe 


K 


Mg 


Na 


Si 


Sr 


Ti 


94 


2.64 


30.4 


1.27 


3.27 


0.45 


0.26 


7.15 


0.17 


0.11 


95 


1.90 


31.6 


1.12 


1.14 


.80 


.29 


6.56 


.03 


.09 


96 


1.72 


27.7 


1.15 


4.44 


.20 


.73 


6.72 


.04 


.09 


97 


2.66 


27.7 


1.74 


2.80 


.32 


.34 


7.34 


.05 


.13 


98 


1.86 


28.1 


1.46 


2.70 


.23 


1.22 


6.52 


.12 


.11 


99 


2.51 


34.1 


1.17 


1.39 


.34 


.18 


4.57 


.04 


.12 


100 


2.39 


27.1 


.93 


5.97 


.33 


.83 


5.77 


.11 


.10 


101 


2.96 


29.8 


1.43 


2.74 


.95 


.18 


8.54 


.06 


.17 


102 


2.45 


34.3 


1.48 


1.98 


.69 


.19 


6.55 


.03 


.12 


103 


2.05 


32.2 


1.81 


1.73 


.56 


.72 


5.67 


.12 


.23 


104 


1.87 


29.3 


1.68 


2.08 


.50 


.14 


7.26 


.03 


.10 


105 


2.05 


31.1 


.96 


2.73 


1.81 


.20 


5.46 


.03 


.09 


106 


2.18 


30.1 


1.06 


3.37 


1.70 


.29 


5.88 


.03 


.11 


107 


2.67 


31.7 


1.13 


1.55 


.36 


.19 


6.59 


.08 


.11 


108 


2.83 


29.8 


1.41 


4.74 


1.61 


.24 


6.53 


.02 


.14 


109 


2.92 


26.1 


4.44 


1.93 


1.38 


.19 


5.40 


.04 


.18 


110 


2.28 


28.2 


.95 


5.09 


.43 


.32 


6.36 


.05 


.11 


111 


2.43 


33.4 


1.35 


2.03 


.68 


.21 


7.33 


.03 


.12 


112 


2.61 


35.2 


1.74 


1.96 


.47 


.10 


7.70 


.09 


.13 


113 


2.53 


36.7 


.88 


4.23 


.54 


.13 


5.91 


.08 


.11 



TABLE 7 . - Trace elements in U.S. cement kiln dust, yg/g^ 



Sample 


Ag 


As 


Cd 


Cr 


Cu 


Li 


Mn 


Ni 


Pb 


Sb 


Zn 


1 


<3 


14 


<1.5 


30 


18 


17 


205 


<12 


<26 


<1.6 


111 


2 


<3 


7.2 


<1.5 


42 


44 


18 


305 


45 


<26 


<1.6 


48 


3 


<3 


23 


6.8 


27 


23 


19 


588 


18 


159 


<1.6 


200 


4 


<3 


5.9 


<1.5 


34 


63 


26 


268 


20 


<26 


<1.6 


214 


5 


<3 


4.3 


<1.5 


29 


19 


25 


414 


23 


43 


<1.6 


50 


6 


<3 


74 


<1.5 


69 


28 


14 


278 


45 


44 


3.0 


118 


7 


<3 


60 


<1.5 


59 


24 


14 


341 


<12 


30 


1.9 


136 


8 


<3 


15 


29 


29 


18 


26 


166 


<12 


569 


<1.6 


455 


9 


<3 


1.6 


12 


32 


28 


76 


180 


72 


1,010 


<1.6 


127 


10 


<3 


28 


<1.5 


51 


26 


58 


334 


32 


366 


<1.6 


171 


11 


<3 


13 


<1.5 


59 


27 


24 


864 


25 


35 


<1.6 


112 


12 


17 


5.7 


<1.5 


62 


23 


56 


166 


20 


91 


1.9 


110 


13 


<3 


1.5 


5.8 


34 


29 


37 


1,330 


<12 


282 


<1.6 


180 


14 


12 


8.0 


<1.5 


51 


28 


71 


111 


<12 


187 


<1.6 


88 


15 


<3 


20 


1.6 


99 


22 


19 


250 


37 


106 


<1.6 


140 


16 


<3 


7.3 


5.8 


41 


18 


33 


202 


24 


<26 


<1.6 


216 


17 


<3 


15 


58 


64 


30 


34 


101 


20 


578 


<1.6 


229 


18 


<3 


9.8 


4.3 


101 


199 


28 


113 


54 


560 


<1.6 


1,330 


19 


<3 


26 


9 


34 


14 


37 


114 


<12 


900 


<1.6 


260 


20 


<3 


14 


11 


116 


17 


16 


63 


31 


84 


1.6 


76 



See footnote at end of table. 



14 



TABLE 7. - Trace elements in U.S. cement kiln dust, Mg/g — Continued 



Sample 


Ag 


As 


Cd 


Cr 


Cu 


Li 


Mn 


Ni 


Pb 


Sb 


Zn 


21 


11 


5.1 


8.6 


29 


27 


<4 


440 


26 


154 


<1.6 


299 


22 


11 


6.3 


22 


48 


30 


23 


489 


33 


204 


1.6 


500 


23 


11 


34 


22 


172 


34 


62 


139 


18 


454 


1.9 


774 


24 


14 


11 


6.4 


47 


57 


18 


204 


34 


278 


3.4 


475 


25 


11 


9.3 


6.2 


35 


18 


<4 


668 


24 


101 


<1.6 


67 


26 


6.7 


8.4 


6.4 


64 


18 


<4 


835 


44 


132 


<1.6 


156 


27 


6.7 


11 


7.7 


43 


18 


<4 


620 


36 


92 


<1.6 


162 


28 


7.0 


14 


5 


18 


56 


<4 


284 


22 


760 


<1.6 


1,860 


29 


6.5 


12 


4.5 


24 


94 


<4 


390 


17 


322 


<1.6 


1,330 


30 


6.5 


8.7 


5.8 


22 


18 


<4 


164 


25 


246 


<1.6 


38 


31 


7.2 


19 


3.2 


34 


24 


<4 


372 


22 


90 


2.7 


54 


32 


5.0 


15 


3.5 


28 


17 


<4 


150 


26 


76 


2.3 


53 


33 


6.0 


7.6 


5 


58 


24 


24 


222 


29 


73 


<1.6 


83 


34 


8.8 


31 


30 


57 


40 


13 


238 


59 


308 


3.9 


1,100 


35 


6.4 


32 


19 


36 


40 


<4 


632 


47 


56 


3.3 


180 


36 


5.9 


20 


8.2 


36 


24 


14 


535 


32 


128 


5.8 


228 


37 


5.0 


6.9 


5 


30 


26 


18 


224 


26 


128 


3.9 


295 


38 


6.6 


6.6 


5.4 


49 


23 


18 


488 


16 


112 


<1.6 


126 


39 


6.6 


4.3 


8.9 


24 


16 


<4 


174 


14 


86 


<1.6 


32 


40 


6.7 


7.6 


6 


120 


20 


7.5 


390 


14 


595 


3.1 


372 


41 


12 


18 


8.9 


32 


42 


14 


439 


34 


161 


<1.6 


167 


42 


11 


6 


6.9 


42 


28 


12 


128 


37 


66 


1.7 


145 


43 


10 


18 


8.2 


31 


27 


23 


1,370 


52 


231 


2.5 


516 


44 


7.5 


7.1 


7.3 


21 


24 


11 


2,410 


41 


223 


<1.6 


155 


45 


8.4 


16 


7.6 


42 


21 


12 


485 


28 


166 


2.2 


952 


46 


6.9 


3.4 


11 


28 


44 


42 


125 


20 


446 


<1.6 


628 


47 


6.4 


8.6 


7.8 


53 


34 


11 


376 


30 


494 


<1.6 


290 


48 


8.8 


3.7 


3.8 


27 


22 


8.2 


244 


22 


35 


<1.6 


105 


49 


8.6 


4.6 


8.8 


90 


54 


<4 


266 


91 


368 


6.7 


391 


50 


6.6 


3 


4.9 


21 


12 


12 


398 


20 


111 


<1.6 


55 


51 


9.8 


17 


8.6 


64 


30 


14 


462 


33 


216 


3.9 


354 


52 


3 


28 


70 


34 


56 


<4 


559 


20 


336 


2.4 


243 


53 


7.3 


29 


6 


30 


26 


<4 


343 


26 


101 


2.7 


220 


54 


9.7 


8.8 


6.4 


40 


52 


<4 


236 


28 


148 


3.8 


8,660 


55 


9.7 


4.3 


9.4 


32 


39 


6.5 


240 


23 


232 


3.7 


2,740 


56 


4.2 


7.1 


8.2 


38 


22 


5 


250 


28 


86 


2.6 


99 


57 


14 


6.5 


20 


77 


22 


21 


176 


18 


1,590 


3 


468 


58 


7.4 


11 


7 


34 


23 


16 


156 


32 


148 


4.4 


144 


59 


14 


4 


62 


31 


28 


22 


408 


28 


964 


<1.6 


158 


60 


11 


2.3 


18 


33 


26 


18 


173 


28 


202 


<1.6 


401 


61 


4.8 


12 


19 


62 


30 


16 


154 


<12 


132 


<1.6 


243 


62 


6.9 


9.5 


<1.5 


36 


27 


16 


252 


12 


76 


<1.6 


58 


63 


6.4 


4.9 


4 


29 


16 


12 


279 


<12 


36 


<1.6 


88 


64 


<3 


7.1 


4 


56 


20 


20 


457 


<12 


420 


<1.6 


167 


65 


<3 


3.4 


45 


28 


16 


22 


90 


<12 


288 


<1.6 


254 


66 


<3 


33 


2.8 


39 


32 


18 


677 


16 


160 


<1.6 


167 


67 


<3 


5.2 


14 


64 


28 


16 


304 


12 


126 


<1.6 


113 


68 


5.3 


3.4 


13 


67 


18 


20 


280 


<12 


94 


<1.6 


75 



^See footnote at end of table. 



TABLE 7. - Trace elements In U.S. cement kiln dust, yig/g — Continued 



15 



Sample 


Ag 


As 


Cd 


Cr 


Cu 


Li 


Mn 


Ni 


Pb 


Sb 


Zn 


69 


4.7 


13 


<1.5 


35 


21 


6 


240 


<12 


54 


<1.6 


71 


70 


7 


44 


6.8 


56 


18 


18 


67 


<12 


221 


<1.6 


199 


71 


5.4 


18 


2.6 


27 


24 


8 


188 


<12 


169 


<1.6 


146 


72 


5.5 


5.8 


<1.5 


43 


22 


16 


141 


<12 


68 


<1.6 


67 


73 


15 


24 


10 


38 


28 


19 


290 


<12 


150 


11 


154 


74 


7.4 


10 


2.6 


37 


54 


32 


239 


17 


98 


<1.6 


206 


75 


12 


509 


42 


48 


56 


14 


534 


24 


260 


29 


702 


76 


12 


518 


42 


47 


64 


14 


542 


24 


258 


27 


714 


77 


6.3 


27 


10 


71 


46 


12 


168 


86 


73 


<1.6 


158 


78 


8.8 


29 


8 


43 


23 


10 


357 


<12 


134 


<1.6 


125 


79 


5.5 


12 


9.5 


33 


18 


17 


424 


<12 


138 


<1.6 


778 


80 


7.9 


25 


5 


47 


34 


8 


236 


14 


31 


<1.6 


129 


81 


<3 


23 


7.8 


43 


46 


47 


1,090 


<12 


272 


<1.6 


703 


82 


<3 


16 


35 


11 


12 


4.2 


136 


<12 


1,240 


<1.6 


115 


83 


13 


77 


16 


28 


206 


9.2 


638 


<12 


1,750 


42 


7,860 


84 


<3 


11 


10 


21 


16 


19 


650 


<12 


204 


<1.6 


134 


85 


<3 


19 


12 


47 


18 


20 


580 


<12 


162 


<1.6 


200 


86 


<3 


15 


2 


33 


14 


26 


456 


<12 


81 


<1.6 


243 


87 


<3 


20 


3.1 


23 


9.4 


11 


592 


<12 


130 


<1.6 


258 


88 


<3 


81 


2.7 


22 


63 


28 


235 


<12 


568 


18 


1,650 


89 


<3 


8 


3.4 


26 


15 


22 


234 


<12 


<26 


2 


53 


90 


<3 


54 


3.4 


23 


36 


21 


350 


<12 


126 


<1.6 


580 


91 


<3 


15 


<1.5 


37 


10 


14 


300 


<12 


39 


<1.6 


32 


92 


<3 


29 


<1.5 


24 


34 


15.6 


274 


<12 


221 


19 


207 


93 


<3 


10 


12 


30 


25 


17 


1,060 


<12 


740 


<1.6 


1,220 


94 


<3 


12 


4.6 


45 


21 


17 


1,250 


<12 


376 


<1.6 


1,060 


95 


<3 


80 


8.8 


16 


29 


7.6 


265 


<12 


426 


70 


792 


96 


<3 


13 


26 


49 


12 


6.6 


370 


<12 


998 


<1.6 


120 


97 


<3 


7.6 


<1.5 


80 


21 


21 


286 


<12 


88 


<1.6 


83 


98 


<3 


1.7 


1.7 


27 


7 


18 


644 


<12 


142 


<1.6 


114 


99 


<3 


2.2 


<1.5 


15 


10 


8.8 


335 


<12 


34 


<1.6 


37 


100 


<3 


2.1 


5 


33 


11 


45 


259 


<12 


56 


1.9 


445 


101 


<3 


3.9 


64 


34 


28 


46 


300 


<12 


144 


<1.6 


516 


102 


<3 


4.7 


16 


18 


7.6 


11 


592 


<12 


80 


2.7 


88 


103 


<3 


1.3 


34 


39 


32 


9.4 


226 


<12 


62 


2 


104 


104 


<3 


4.2 


16 


35 


8.3 


7.4 


302 


<12 


66 


2.7 


83 


105 


<3 


2.9 


352 


26 


14 


8.4 


280 


<12 


182 


<1.6 


88 


106 


<3 


2.8 


305 


23 


18 


9.4 


266 


<12 


206 


<1.6 


108 


107 


<3 


2.3 


100 


18 


14 


10 


820 


<12 


362 


<1.6 


398 


108 


<3 


11 


24 


35 


24 


16 


410 


<12 


150 


<1.6 


150 


109 


<3 


4.6 


18 


30 


34 


19 


336 


<12 


542 


1.8 


207 


110 


<3 


3.1 


81 


18 


12 


55 


177 


<12 


182 


1.9 


322 


111 


<3 


1.9 


9.9 


14 


12 


6.9 


198 


<12 


38 


<1.6 


58 


112 


<3 


1.7 


66 


15 


13 


8.2 


203 


<12 


28 


2.9 


38 


113 


<3 


3 


141 


18 


16 


10 


248 


<12 


72 


1.8 


79 



^Elements not detected in any of the samples: 

Ba <55; Be <2; Bi <50; Co <10; Mo <50; Sn <100; V <100. 



16 



TABLE 8. - Elemental and anion variation In U.S. cement kiln dust, lig/g 



Element or anion 



Range 



Mean 



Median 



Ag. 
Al. 
As. 
Ba. 
Be. 
Bi. 
Ca. 
Cd. 
Co. 
Cr. 
Cu. 
Fe. 
Hg2 
K.. 
Li. 
Mg. 
Mn. 
Mo. 
Na. 
Ni. 
Pb. 
Sb. 
Si. 
Sn. 
Sr. 
Ti. 
Tl. 
V . 
Zn. 
Br~ 
CI" 
F~. 
NO2 
NO3 
PO4 
SO4 



3-. 
1- 



<3 


17 


9,900 


- 50,200 


1.3 


518 


<55 




<2 




<50 




06,000 


-367,000 


<1.5 


352 


<10 




11 


172 


7 


206 


1,000 


- 44,400 


<0.13- 1.0 


3,400 


-232,000 


<4 


76 


1,980 


- 19,100 


63 


- 2,410 


<50 




495 


- 27,700 


<12 


91 


17 


- 1,750 


<1.6 


70 


26,900 


-111,000 


<100 




62 


- 8,750 


500 


- 2,900 


<60 


185 


<100 




32 


- 8,660 


<200 




<100 


-123,000 


100 


- 3,600 


<200 




200 


- 16,700 


200 


- 1,600 


4,100 


-316,000 



5.4 

23,200 

24 

<55 

<2 

<50 

295,000 

21 

<10 

41 

30 

14,700 

<.13 

36,600 

18 

7,820 

383 

<50 

4,700 

22 

253 

3.2 

63,500 

<100 

670 

3,530 

<60 

<100 

462 

<200 

6,900 

1,300 

<200 

<200 

<200 

77,800 



4.8 
23,100 

9.3 

<55 

<2 

<50 

305,000 

7.3 

<10 

34 

24 

14,100 

<.13 

26,800 

16 

6,820 

280 

<50 

3,190 

29 

148 

<1.6 

65,100 

<100 

430 

1,100 

<60 

<100 

167 

<200 

4,900 

1,000 

<200 

<200 

<200 

68,600 



^A value of 1/2 the 
the mean for those 
detection limit. 



detection limit was arbitrarily used 
elements having concentrations both 



to calculate 
above and below the 



^Mercury value based on only 16 samples. 



17 



TABLE 9. - Mercury in selected U.S. 
cement kiln dust samples, Ug/g 



Sample 


Mercury 


Sample 


Mercury 


8 

9 

13 

14 

17 

19 

35 

49 


<0.13 
1.0 

.13 
<.13 
<.13 
<.13 

.63 
<.13 


52... 

58... 

64... 

65... 

68... 
104... 
108... 
110. .. 




0.25 
.13 

<.13 
.38 

<.13 

1.0 

<.13 
.63 



Interelement Correlations 

Interelement correlation coeffici- 
ents were generated using linear regres- 
sion analysis on a total of 23 elements, 
anions, carbonate carbon as CO2, noncar- 
bonate carbon, and chemically bound 
water. Coefficients with values r >0.4 
or r <-0.4 were taken as significant 
positive or negative correlations. Of 
the 23 parameters tested, only 14 para- 
meters showed significant correlation. 
Table 10 shows the interelement correla- 
tion coefficients for the 23 pairs. 
Some very significant correlations 



TABLE 10. - Interelement correlation coefficients for U.S. cement kiln dust 



Element or anion 


Al 


Ca 


ci- 


CO 


F- 


Fe 


K 


Al 


1 










0.46 




Ca 




1 


-0.45 








-0.85 


Cl~ 




-.45 


1 


1 


-0.42 




.56 


CO 




F" 








-.42 


1 






Fe 


.46 










1 




K 




-.85 


.56 








1 


Li 




-.54 










.44 


Na 




-.55 






.42 




.47 


Pb 




-.42 












Si 


.48 












-.55 


Sr 
















SO 2- 

Ti? 




-.77 




-.51 






.77 


.77 










.49 






Li 


Na 


Pb 


Si 


Sr 


S0^2- 


Ti 


Al 








0.48 






0.77 


Ca 


-0.54 


-0.55 


-0.42 




-0.77 


-0.77 




Cl~ 
















CO 












-.51 




F~ 




.42 












Fe 


.49 


K 


.44 


.47 




-.55 




.77 




Li 


1 


.41 








.49 




Na 


.41 


1 






0.52 






Pb 






1 










Si 








1 




-.44 


.42 


Sr 


.49 


.52 


-.44 


-.44 
.42 


1 


1 








Ti 


1 



■■^Blank indicates that correlation coef ficient is insignificant (-0.4 < r <0.4) 



18 



(r>0.7, r<-0.7) were found for Al and Ti 
(r = 0.77), Ca and K (r = -0.85), Ca and 



SO, 



2- 



(r = -0.77), and K and 



S0^2- 



(r = -0.77). Chlorine and potassium 
(the mineral sylvite, KCl) showed a 
positive correlation coefficient of 



r = 0.56. The remaining parameters of 
As, noncarbonate carbon, Cd, Cr, Cu, 
chemically bound water, Mg, Mn, and Zn 
had no significant correlations with any 
of the other parameters. 



EPA HAZARDOUS WASTE TEST 



According to EPA regulations, a 
solid waste must be listed as hazardous 
if it exhibits ignitability, corrosivi- 
ty, reactivity, or toxicity, using the 
extraction procedure outlined in the 
Federal Register (4^-5^) . CKD does not 
meet the criteria for a hazardous waste 
under ignitability, corrosivity, or 
reactivity. Briefly, the EP toxicity 
test as applied to CKD in this study 
consisted of adding 100 grams of CKD to 
1,600 ml of distilled water, gradually 
adding 400 ml of 0.5-normal acetic acid, 
and agitating for 24 hours. Although 
400 ml of acetic acid was the maximum 
amount specified by the test procedure, 
the pH never approached the specified pH 
of 5 +0.2. The resulting extract in the 
EP toxicity test must not exceed 100 
times the National Drinking Water Stand- 
ard with respect to the concentration of 
eight metals: As, Ba, Cd, Cr, Pb, Hg, 
Se, and Ag. Tgble 11 lists the allowed 
maximum concentrations. Only one sample 
exceeded any of the limits; this sample 
(83) exceeded the 5-ug/ml lead 
limit with an average of 15 Ug/ml 
in duplicate runs. Sample 83 contained 
the highest lead value of the 113 
samples, but this concentration is still 
a factor of 3 less than the concentra- 
tion reported in the West German sample 
(3). 



Additional supplies of sample 83 could 
not be obtained from the plant to see if 
this high lead value was anomalous. The 
highest zinc level was found in sample 
54 with a concentration of 8,660 
pg/g, which is a factor of 2 less 
than the value reported for the West 
German sample . Although zinc is not a 
factor in the EP toxicity tests, it is 
of environmental interest. 



TABLE 11. - Maximum concentration of 



contaminants allowed for EP 
toxicity test (4 5) 



EPA hazardous 
waste number 


Contaminant 


Maximum 
concen- 
tration 
yg/ml 


D004 

D005 

D006 

D007 

D008 

D009 

DOlO 


Arsenic. . . . 

Barium 

Cadmium. . . . 
Chromium. . . 

Lead 

Mercury. . . . 
Selenium. . . 
Silver 


5.0 
100.0 
1.0 
5.0 
5.0 
.2 
1.0 


DOll 


5.0 



SUMMARY AND CONCLUSIONS 



As part of the Bureau of Mines ' min- 
erals environmental technology program, 
the Avondale Research Center has comple- 
ted an extensive characterization of 
dusts generated from U.S. cement kilns. 
Because of the interest of the EPA and 
Congress (4-_5, 10 ) in CKD as a large- 
volume waste of unknown environmental 



impact, the mineralogical and chemical 
compositions and the hazardous waste 
potential of CKD were investigated. 
Data from mineralogical analysis show 
that the major constituents of CKD are 
calcite, lime, and anhydrite with vary- 
ing amounts of quartz and dolomite. 



19 



A total of 28 elements was deter- 
mined in 113 CKD samples. In addition, 
seven anion species, carbon dioxide, 
noncarbonate carbon, and chemically 
bound water were determined in all sam- 
ples. Mercury was determined in 16 
selected samples. 

Chemical analyses show 13 elements 
or anion species occurring in CKD at 
concentrations consistently greater than 
0.05 wt-pct. These constituents are Al, 
Ca, CI", CO2, F", Fe, K, Mg, Na, 
Si, SO42", Sr, and Ti. The upper 
range limits for heavy metal concentra- 
tions such as lead and zinc are a factor 
of 2 or 3 less than the value reported 



for a CKD sample from Blaubeuren, West 
Germany (3) . 

The U.S. Environmental Protection 
Agency EP toxicity test was performed on 
all samples. Only 1 of the 113 samples 
had a leachate concentration that ex- 
ceeded any of the limits; it slightly 
exceeded the criterion for lead. 

Cement kiln dust is a large-volume 
material and a potential resource as a 
substitute for lime. Any environmental 
considerations are minor, as the results 
of this extensive survey show that U.S. 
CKD is not a hazardous waste as defined 
by current regulations established under 
RCRA. 



REFERENCES 



1. Agemian, H. , and A. S. Y. Chau. 
An Improved Digestion Method for the 
Extraction of Mercury From Environmental 
Samples. Analyst, v. 101, 1976, pp. 
91-95. 

2. A. T. Kearney, Inc. Multimedia 
Assessment and Environmental Research 
Needs of the Cement Industry. Contract 
68-03-2586, Work Directive 2586-WDl , 
USEPA G-195, 1979, 84 pp. 

3. Davis, T. A., and D. B. Hooks. 
Disposal and Utilization of Waste Kiln 
Dust From Cement Industry. EPA-670/2- 
75-043, 1975, 54 pp. 

4. Federal Register. Part IV, Envi- 
ronmental Protection Agency: Hazardous 
Waste; Proposed Guidelines and Regula- 
tions and Proposal on the Identification 
and Listing. V. 43, No. 243, Dec. 18, 
1978, pp. 58946-59028; 110 CFR, Part 
250. 

5. . Parts II-IX, Environmen- 
tal Protection Agency: Hazardous Waste 
and Consolidated Permit Regulations. V. 
115, No. 98, May 19, 1980, Book 2, pp. 
33063-33285; 110 CFR, Parts 260-265. 

6. Haynes, B. W. Electrothermal 
Atomic Absorption Determination of 
Arsenic and Antimony in Combustible 



Municipal Solid Waste. Atomic Absorp- 
tion Newsletter, v. 17, No. 3, 1978, pp. 
49-52. 

7. Haynes, B. W. , G. W. Kramer, and 
J. A. Jolly. Fluorine and Uranium in 
Phosphate Rock Processing and Waste Ma- 
terials. BuMines RI 8576, 1981, 17 pp. 

8. Haynes, B. W. , S. L. Law, and J. 
A. Jolly. Eastern Cement Kiln Dust Char- 
acterization. Pres. at 110th AIME Ann. 
Meeting, Chicago, 111., Feb. 22-26, 1981, 
TMS Preprint A81-39, 10 pp. 

9. Haynes, B. W. , J. C. McConnell, 
and S. L. Law. Antimony, Arsenic and 
Mercury in the Combustible Fraction of 
Municipal Solid Waste. BuMines RI 8293, 
1978, 11 pp. 

10. U.S. Congress. Conference Report 
on S. 1156, Solid Waste Disposal Act 
Amendments. Congressional Record 
House, Oct. 1, 1980, pp. H10174-H10187 . 

11. . Resource Conservation and 
Recovery Act of 1976, Public Law 94-580, 
Oct. 21, 1976. 

12. Wheeler, W. E., and R. R. Oltjen. 
Cement Kiln Dust in Diets for Finishing 
Steers. U.S. Dept. Agriculture, Agricul- 
tural Research Service, ARS-NE-88 , 9 pp. 



INT.-BU.OF MINI ES,PGH..P A. 26379 



H 64 83 



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